CN106374137B - A kind of kalium ion battery organic cathode material and preparation method thereof - Google Patents
A kind of kalium ion battery organic cathode material and preparation method thereof Download PDFInfo
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- CN106374137B CN106374137B CN201610827234.2A CN201610827234A CN106374137B CN 106374137 B CN106374137 B CN 106374137B CN 201610827234 A CN201610827234 A CN 201610827234A CN 106374137 B CN106374137 B CN 106374137B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention provides a kind of novel kalium ion battery organic cathode materials, its active material is organic carboxyl acid sylvite, preparation method is that organic matter carboxylic-containing acid is reacted ultrasonic mixing with potassium hydroxide, then 24-72h is reacted in 100-120 DEG C of sealing, then addition solvent makes its precipitating, is finally centrifuged, cleans, is dry obtained.The negative electrode material shows reversible deintercalation potassium ion platform, and outstanding cycle performance has excellent potassium ion and electron propagation ducts, and crystal structure is stable in the electrolytic solution and synthetic method is simple, environmentally protective, can be prepared as flexible battery.Such novel kalium ion battery can effectively solve the problems such as environmental pollution caused by the shortage of resources of lithium ion battery electrode material, transition metal use.
Description
Technical field
The invention belongs to ion battery technology fields, and in particular to a kind of novel kalium ion battery organic cathode material and its
Preparation method.
Background technique
With the continuous development of modern society, scientific and technological progress, traditional fossil energy such as coal, petroleum, natural gas etc. is deposited
It is limited in resource, the drawbacks such as pollute the environment, therefore energy crisis becomes increasingly conspicuous with the problems such as environmental pollution, traditional change
The stone energy is far from satisfying requirement of the mankind to green clean energy resource society is constructed.Consequent is with new technology and green wood
Based on material, the development and utilization for modernizing traditional renewable resource can effectively solve above situation.For exploitation
New energy it is varied, such as wind energy, nuclear energy, solar energy, biological energy source, geothermal energy, tide energy.For opening for these new energy
It sends out and improves unified theoretical system using needing to establish, wherein energy storage is exactly a wherein critically important step.
Energy storage depend on relevant energy storage material and device, storage and conversion element of the lithium ion battery as the energy,
New energy field occupies an important position, but the lithium resource reserves in the earth's crust are extremely limited, while inorganic material used in lithium battery
The problems such as expecting that there are toxic transition metal, this generates very big pollution to environment, therefore develops environmentally protective recyclable
Secondary cell has very big realistic meaning.In recent years, many novel substitution energy-storage batteries come into being, and rapidly develop, mainly
Including secondary cells such as sodium ion, potassium ion, magnesium ion, calcium ions.Kalium ion battery has many advantages, wherein potassium resource price
Cheaply, the normal reduction potential of the rich content in the earth's crust, kalium ion battery and lithium ion battery is closest thus energy
Metric density is high, and kalium ion battery electrolyte electrochemical activity height is conducive to the transmission of ion and electronics.Potassium reported at present
Ion battery cathode material is less, and wherein there is carbon material lower deintercalation potassium current potential dendrite easy to form to cause security risk.
Therefore environmentally protective, stable structure is developed, electrochemistry deintercalation potassium platform is suitable, the big novel organic kalium ion battery tool of specific capacity
It is of great significance.
Summary of the invention
For the above-mentioned problems in the prior art, the present invention provides a kind of novel organic cathode material of kalium ion battery
Material, preparation method is simple, such material has environmentally protective, can be recycled, stable structure, with excellent three-dimensional ion
And electron propagation ducts, it can be used as the substitute of lithium ion battery.
To achieve the above object, the technical solution adopted by the present invention to solve the technical problems is：
The active material of a kind of kalium ion battery organic cathode material, the negative electrode material is organic carboxyl acid potassium, and general formula is formula
Ⅰ：
Wherein, carboxylic acid potassium base (- COOK) number is at least 2, and R is phenyl ring, pyridine ring, pyridine ring or pyrimidine ring.
Further, the H on R can be taken by one or more of fluorine, chlorine, bromine, iodine, nitro, amino, hydroxyl and carboxyl
Generation；Wherein the H in hydroxyl and carboxyl can also be replaced by potassium.
Further, position of the carboxylic acid potassium base (- COOK) on R is：Ortho position, meta or para position.
The preparation method of above-mentioned kalium ion battery organic cathode material, includes the following steps：
It (1) is in molar ratio 1 by organic matter carboxylic-containing acid and potassium hydroxide:2-4 mixing, is then dissolved in water or alcohol, surpasses
Sound stirs 1-1.5h；
(2) reaction solution obtained by step (1) is placed in 100-120 DEG C of sealing reaction 24-72h；
(3) solvent is added into step (2) gained reactant and generates precipitating to complete, is then centrifuged for, cleans, finally by institute
It obtains solid and is placed in 60-80 DEG C of dry 6-8h, then in 100-120 DEG C of vacuum drying 3-6h, obtain the organic cathode material of kalium ion battery
Material.
Further, the alcohol in step (1) is dehydrated alcohol.
Further, the solvent in step (3) is dehydrated alcohol, acetone or DMF.
A kind of kalium ion battery organic cathode material provided by the invention and preparation method thereof, has the advantages that：
(1) kalium ion battery organic cathode material made of the present invention can effectively solve the problem that lithium ion battery scarcity of resources is asked
Topic has more stable structure compared with lithium salts and sodium salt, and solubility in the electrolytic solution is lower, and the transmission of three-dimensional ion is logical
Road is bigger, is suitble to the transmission of potassium ion, and the performance such as organic acid, lithium salts, sodium salt is poor or without reversible deintercalation potassium ion performance.
(2) kalium ion battery organic cathode material prepared by the present invention has excellent charge-discharge performance, coulombic efficiency
Height, good cycling stability, specific capacity are high.
(3) compared with inorganic material, organic carboxyl acid sylvite can be used for preparing organic flexible electrode material.
Detailed description of the invention
Fig. 1 is the SEM spectrum of potassium terephthalate prepared by embodiment 1.
Fig. 2 is X-ray diffraction (XRD) map of potassium terephthalate prepared by embodiment 1.
Fig. 3 is that potassium terephthalate prepared by embodiment 1 is applied to kalium ion battery, and current density is the list under 44mA/g
All charging and discharging curve figures.
Fig. 4 is that potassium terephthalate prepared by embodiment 1 is applied to kalium ion battery, and current density is following under 44mA/g
Ring performance map.
Fig. 5 is that potassium terephthalate prepared by embodiment 1 is applied to kalium ion battery, and current density is can under 44mA/g
Inverse charging and discharging curve figure.
Fig. 6 is the SEM spectrum of pyridine -2,5- dicarboxylic acids potassium prepared by embodiment 2.
Fig. 7 is X-ray diffraction (XRD) map of pyridine -2,5- dicarboxylic acids potassium prepared by embodiment 2.
Fig. 8 is that pyridine -2,5- dicarboxylic acids potassium prepared by embodiment 2 is applied to kalium ion battery, current density 44mA/g
Under single-revolution charging and discharging curve figure.
Fig. 9 is that pyridine -2,5- dicarboxylic acids potassium prepared by embodiment 2 is applied to kalium ion battery, current density 44mA/g
Under cycle performance figure.
Figure 10 is that pyridine -2,5- dicarboxylic acids potassium prepared by embodiment 2 is applied to kalium ion battery, current density 44mA/g
Under reversible charging and discharging curve figure.
Figure 11 is in comparative example using 2,5-Dihydroxyterephthalic acid as kalium ion battery negative electrode material, and current density is
Charging and discharging curve figure under 20mA/g.
Figure 12 is in comparative example using 2,5-Dihydroxyterephthalic acid as kalium ion battery negative electrode material, and current density is
Cycle performance figure under 20mA/g.
Specific embodiment
Embodiment 1
A kind of preparation method of kalium ion battery organic cathode material, includes the following steps：
(1) terephthalic acid (TPA) and the pure KOH of 3.05g analysis that 2g purity is 99% are weighed respectively, are then added and 40mL is housed
In the flask of deionized water, with magnetic stirrer 1h；
(2) reaction solution obtained by step (1) is transferred in polytetrafluoroethylliner liner, and sealed in a kettle, 110
72h is reacted under the conditions of DEG C；
(3) step (2) gained reactant 20mL is measured, 50mL dehydrated alcohol is added, obtains white precipitate, is then centrifuged for,
It is cleaned 3 times or more with deionized water, obtained solid is placed in 60 DEG C of dry 8h, then in 110 DEG C of vacuum drying 6h, it is organic right to obtain
Phthalic acid potassium negative electrode material.
Potassium terephthalate (K2TP it) is used as potassium ion negative electrode material, reversible deintercalation potassium mechanism is as follows：
From the foregoing, it will be observed that conjugation carboxylic acid potassium base can realize reversible opening state in the insertion of potassium ion and abjection process,
The transmission channel of three-dimensional ion and electronics is provided.
The K prepared by above-mentioned preparation method2TP, scanning electron microscope (SEM) map are shown in Fig. 1, as shown in Figure 1,
The material as made from simple chemical synthesis process is micron particles, can further prepare nanometer by modes such as ball millings
Grain.
X-ray diffraction (XRD) map of potassium terephthalate is shown in Fig. 2, and as shown in Figure 2, potassium terephthalate is crystallinity
Good material shows apparent high preferred orientation.
Using potassium terephthalate as negative electrode material assemble kalium ion battery, using KFSI (double fluorine sulfimide sylvite) as
Electrolyte, specific step is as follows：Electrode slice is made in potassium terephthalate, as the negative electrode material of kalium ion battery, is carried out
Half-cell assembles, wherein the mass ratio of active material, acetylene black, PVDF (polytetrafluoroethylene (PTFE)) (solvent is N-Methyl pyrrolidone)
It is 6:3:1, metallic potassium is to battery, and glass fibre membrane is diaphragm, and electrolyte is that the KFSI of 1mol/L is dissolved in EC (ethylene carbonate
Ester) and DMC (dimethyl carbonate) by volume be 1:In 1 mixed solution, cycle performance survey is carried out to the battery that assembling obtains
Examination, current density 44mA/g, reversible single-revolution charging and discharging curve figure are shown in Fig. 3, and cycle performance figure is shown in Fig. 4, reversible charge and discharge
Electric curve graph is shown in Fig. 5.
By Fig. 3, Fig. 4 and Fig. 5 it is found that the kalium ion battery shows apparent charge and discharge platform, electric discharge and charging platform
In the position of 0.5/0.7V, it can effectively solve carbon material hypopotenia and form the safety issues such as dendrite, suitable voltage is flat
Platform can also improve the power density of material, and therefore, potassium terephthalate prepared by the present invention is highly suitable as potassium ion electricity
Pond negative electrode material.The reversible charge specific capacity of the battery is 189mAh/g, and up to 98% or more, which has excellent coulombic efficiency
Cycle performance.Compared with organic terephthalic acid (TPA), lithium salts and sodium salt, the transmission with optimal three-dimensional ion and electronics is logical
Road, and its solubility in the electrolytic solution is lower, and chemical stability is more preferable, solves the solubility problem of material, simultaneously also
With reversible deintercalation potassium ion performance.
Kalium ion battery is assembled using potassium terephthalate as negative electrode material, with KPF6(Potassium Hexafluorophosphate) is as electrolysis
Matter, specific step is as follows：Electrode slice is made in potassium terephthalate, as the negative electrode material of kalium ion battery, carries out half electricity
Pond assembling, wherein active material, acetylene black, PVDF (solvent is N-Methyl pyrrolidone) mass ratio be 6:3:1, metallic potassium is
To battery, glass fibre membrane is diaphragm, and electrolyte is the KPF of 0.5mol/L6It is dissolved in EC and DMC is 1 by volume:1 it is mixed
It closes in solution, cycle performance test is carried out to the battery that assembling obtains, also shows reversible potassium ion deintercalation performance.
Embodiment 2
A kind of preparation method of kalium ion battery organic cathode material, includes the following steps：
(1) weigh pyridine -2,5- dicarboxylic acids that 2g purity is 99% respectively and 3.05g analyze pure KOH, mixing, then plus
Enter in the flask equipped with 40mL deionized water, with magnetic stirrer 1h；
(2) reaction solution obtained by step (1) is transferred in polytetrafluoroethylliner liner, and sealed in a kettle, 110
72h is reacted under the conditions of DEG C, obtains clear solution；
(3) step (2) gained reactant 20mL is measured, 50mL dehydrated alcohol is added, obtains white precipitate, is then centrifuged for,
It is cleaned 3 times or more with deionized water, obtained solid is placed in 80 DEG C of dry 6h, then in 120 DEG C of vacuum drying 6h, obtains pyridine-
2,5- dicarboxylic acids potassium (K2C7H3NO4) negative electrode material.
For pyridine -2,5- dicarboxylic acids potassium as potassium ion negative electrode material, reversible deintercalation potassium mechanism is as follows：
Pyridine -2, the 5- dicarboxylic acids potassium prepared by above-mentioned preparation method, scanning electron microscope (SEM) map are shown in figure
6, X-ray diffraction (XRD) map is shown in Fig. 7.
Pyridine -2,5- dicarboxylic acids potassium is assembled into kalium ion battery as negative electrode material, it is specific using KFSI as electrolyte
Steps are as follows：Electrode slice is made in pyridine -2,5- dicarboxylic acids potassium, as the negative electrode material of kalium ion battery, carries out half-cell group
Dress, wherein active material, acetylene black, PVDF (solvent is N-Methyl pyrrolidone) mass ratio be 6:3:1, metallic potassium is to electricity
Pond, glass fibre membrane are diaphragm, and the KFSI that electrolyte is 1mol/L is dissolved in EC and DMC is 1 by volume:1 mixed solution
In, cycle performance test, current density 44mA/g are carried out to the battery that assembling obtains, single-revolution charging and discharging curve figure is shown in Fig. 8,
Cycle performance figure is shown in Fig. 9, and reversible charging and discharging curve figure is shown in Figure 10.
By Fig. 8, Fig. 9 and Figure 10 it is found that the kalium ion battery shows apparent charge and discharge platform, electric discharge and charging platform
In the section of 0.6-0.7/0.8-0.9V, the safety issue of carbon material can effectively solve, suitable voltage platform can also
The power density of material is enough improved, therefore, pyridine -2,5- dicarboxylic acids potassium prepared by the present invention is highly suitable as kalium ion battery
Negative electrode material.The reversible charge specific capacity of the battery is 191mAh/g, and up to 98% or more, which has excellent coulombic efficiency
Cycle performance.Compared with organic acid, lithium salts and sodium salt, the transmission channel with bigger three-dimensional ion and electronics, and its
Solubility in the electrolytic solution is lower, solves the solubility problem of material, while also having reversible deintercalation potassium ion performance.
Comparative example 1
Kalium ion battery is assembled using 2,5-Dihydroxyterephthalic acid as negative electrode material, using KFSI as electrolyte,
Specific step is as follows：Electrode slice is made in 2,5-Dihydroxyterephthalic acid, as the negative electrode material of kalium ion battery, carries out half
Battery assembly, wherein active material, acetylene black, PVDF (solvent is N-Methyl pyrrolidone) mass ratio be 6:3:1, metallic potassium
For to battery, glass fibre membrane is diaphragm, and the KFSI that electrolyte is 1mol/L is dissolved in EC and DMC is 1 by volume:1 it is mixed
It closes in solution, cycle performance test, current density 20mA/g is carried out to the battery that assembling obtains, charging and discharging curve figure is shown in figure
11, cycle performance figure is shown in Figure 12.
As shown in Figure 11, which does not show apparent charge and discharge platform, as shown in Figure 12, reversible charging specific volume
Amount is 80mAh/g, and compared to sylvite such as organic potassium terephthalate, pyridine -2,5- dicarboxylic acids potassium, organic carboxyl acid is as potassium ion
Cell negative electrode material fails to show excellent deintercalation potassium ion performance, this is mainly and in the molecular structure of organic carboxyl acid, although
It is capable of providing transmission lithium ion and sodium-ion channel, but since potassium ion radius is larger, needs to overcome bigger potential barrier, therefore have
Machine carboxylic acid shows poor chemical property as kalium ion battery negative electrode material.
Comparative example 2
Kalium ion battery, using KFSI as electrolyte, specific steps are assembled using terephthalic acid (TPA) lithium as negative electrode material
It is as follows：Electrode slice is made in terephthalic acid (TPA) lithium, as the negative electrode material of kalium ion battery, half-cell assembling is carried out, wherein living
Property substance, acetylene black, PVDF (solvent is N-Methyl pyrrolidone) mass ratio be 6:3:1, metallic potassium is to battery, glass fibers
Dimension film is diaphragm, and the KFSI that electrolyte is 1mol/L is dissolved in EC and DMC is 1 by volume:In 1 mixed solution, to assembling
Obtained battery carries out cycle performance test, fails to show electro-chemical activity, compared with potassium salt, organic carboxyl acid lithium salts
Fail to show the performance of reversible deintercalation potassium ion as kalium ion battery negative electrode material, it is right since potassium ion radius is larger
The molecular structure of phthalic acid lithium cannot provide its transmission channel, be unable to electrochemistry storage potassium, therefore, such lithium salts cannot function as potassium
Ion secondary battery electrode material.
Claims (2)
1. a kind of preparation method of kalium ion battery organic cathode material, which is characterized in that include the following steps：
It (1) is in molar ratio 1 by organic matter carboxylic-containing acid and potassium hydroxide:2-4 mixing, is then dissolved in water or alcohol, ultrasound is stirred
Mix 1-1.5h；Wherein, organic matter carboxylic-containing acid is terephthalic acid (TPA) or pyridine -2,5- dicarboxylic acids；Alcohol is dehydrated alcohol；
(2) reaction solution obtained by step (1) is placed in 100-120 DEG C of sealing reaction 24-72h；
(3) solvent to complete reaction is added into step (2) gained reactant and obtains sediment, is then centrifuged for, cleans, finally will
Obtained solid is placed in 60-80 DEG C of dry 6-8h, and then in 100-120 DEG C of vacuum drying 3-6h, it is organic negative to obtain kalium ion battery
Pole material；Wherein, solvent is dehydrated alcohol, acetone or DMF.
2. the kalium ion battery organic cathode material that the method according to claim 11 is prepared.
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| CN106410148B (en) * | 2016-10-28 | 2019-03-19 | 南开大学 | A kind of high-performance kalium ion battery negative electrode material and the electrolyte to match |
| CN107275601B (en) * | 2017-06-02 | 2020-01-07 | 电子科技大学 | Aromatic hyperconjugated dicarboxylate and application of graphene composite material thereof |
| CN107331866A (en) * | 2017-06-23 | 2017-11-07 | 山东大学 | A kind of application of expanded graphite in kalium ion battery negative material |
| CN107275578B (en) * | 2017-07-05 | 2020-09-22 | 中国矿业大学 | Method for manufacturing potassium ion battery cathode by adopting nitrogen-doped porous carbon material |
| CN108091831B (en) * | 2017-11-10 | 2020-10-27 | 浙江衡远新能源科技有限公司 | Preparation method of lithium ion battery negative electrode material, negative electrode material and lithium ion battery |
| CN108258244B (en) * | 2018-01-25 | 2022-10-21 | 电子科技大学 | Novel lithium ion/potassium ion battery negative electrode material and preparation method thereof |
| CN110277558B (en) * | 2018-03-15 | 2022-04-08 | 上海大学 | Lithium ion battery cathode material and preparation method thereof |
| CN110416528A (en) * | 2018-04-27 | 2019-11-05 | 广东工业大学 | A kind of kalium ion battery |
| CN111952586A (en) * | 2020-07-10 | 2020-11-17 | 西安理工大学 | High first-cycle coulombic efficiency potassium ion battery organic carbonyl negative electrode material and preparation method thereof |
| CN111952587A (en) * | 2020-07-24 | 2020-11-17 | 西安理工大学 | Organic carbonyl electrode material of high-capacity potassium ion battery and preparation method thereof |
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